CN109485434A - The method of low temperature synthesis yttrium-aluminium-garnet ceramic powder - Google Patents
The method of low temperature synthesis yttrium-aluminium-garnet ceramic powder Download PDFInfo
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- CN109485434A CN109485434A CN201910044851.9A CN201910044851A CN109485434A CN 109485434 A CN109485434 A CN 109485434A CN 201910044851 A CN201910044851 A CN 201910044851A CN 109485434 A CN109485434 A CN 109485434A
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- 239000000843 powder Substances 0.000 title claims abstract description 103
- 239000002223 garnet Substances 0.000 title claims abstract description 44
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 40
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 23
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000004576 sand Substances 0.000 claims abstract description 18
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 239000008188 pellet Substances 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 7
- 229920000193 polymethacrylate Polymers 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000003701 mechanical milling Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 16
- 239000002609 medium Substances 0.000 description 9
- 238000005245 sintering Methods 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 229920002635 polyurethane Polymers 0.000 description 7
- 239000004814 polyurethane Substances 0.000 description 7
- 239000008187 granular material Substances 0.000 description 6
- 238000003801 milling Methods 0.000 description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007780 powder milling Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 229910001679 gibbsite Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
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- 239000011858 nanopowder Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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Abstract
The present invention relates to a kind of methods of low temperature synthesis yttrium-aluminium-garnet ceramic powder, comprising steps of rare earth oxide and aluminum contained compound are placed in agitating ball mill, with the speed ball milling 1-2h of 130-150r/min, cross 80 meshes later, obtain powder；Wherein, rare earth oxide Y2O3Or Er2O3And Y2O3The mixture of the two；Powder is put into sand mill, 3-4h is ground with the revolving speed of 2200-2700r/min, filtering means dehydration and dries later, obtains the superfine powder that grain diameter is 20-50nm；By superfine powder 1100-1200 DEG C heat preservation 5-7 hours, obtain yttrium-aluminium-garnet ceramic powder.The yttrium-aluminium-garnet ceramic powder chemical composition stability that the present invention is prepared is single garnet structure, and size distribution is at 20-120 μm.
Description
Technical field
The present invention relates to field of material technology, and in particular to a kind of method of low temperature synthesis yttrium-aluminium-garnet ceramic powder.
Background technique
Yttrium-aluminium-garnet Y3Al5O12(YAG) there is excellent thermal property and thermal stability, so being considered as that thermal boundary applies
A kind of potential candidate of layer material.Studies have shown that carrying out Y using rare earth element (Gd, Er, Yb etc.)3+Position doping can be into one
Step improves Y3Al5O12Thermophysical property, such as utilize Er3+Part replaces Y3+Position, can effectively reduce the thermal conductivity of yttrium-aluminium-garnet
Rate.
Currently, YAG raw powder's production technology mainly have solid phase method, sol-gel method (Sol-gel), solvent (water) thermal method,
Coprecipitation, mechanochemical synthesis, spray pyrolysis obtain superfine powder using above method, then pass through 1600 DEG C of high temperature
The above normal pressure or vacuum-sintering obtain yttrium-aluminium-garnet ceramic powder.However yttrium-aluminium-garnet ceramic powder is prepared using above method
When body, have the following defects.When preparing powder using sol-gel method, the Organic Ingredients cost as used in sol-gel method
Height, reaction process is not easy to control, and the YAG aqueous precursor gel prepared washs difficulty, easily forms second particle, presoma when dry
It can cause the hard aggregation of powder granule in heat treatment, so that the dispersibility for finally preparing powder is poor, sintering activity is undesirable,
Fail to obtain the good ceramic body material of the transparency.When preparing powder using solvent-thermal process method, since this method is to equipment etc.
Condition requires stringent, high production cost, so being unsuitable for producing in batches.Solid phase method is a kind of common powder preparation method, benefit
Raw material ball milling 20-24h is uniformly mixed with general milling method and powder of the granularity at 1-10 μm, this method have technique letter
The advantages that single, high-efficient, at low cost, easy batch production；However the powder obtained using solid phase method is when synthesizing yttrium-aluminium-garnet,
Since big, the active low and mixing uniformity of mixture powder granularity that general ball milling solid phase method obtains is poor, synthesis temperature
Height, soaking time is long, needs vacuum-sintering, and generally requiring could synthesize or 1800 DEG C or more in 1600 DEG C of heat preservation 20h or more
Vacuum-sintering, process conditions require and high production cost, and the properties of powder synthesized is unsatisfactory.
Summary of the invention
For the defects in the prior art, it is an object of that present invention to provide a kind of low temperature to synthesize yttrium-aluminium-garnet ceramic powder
Method, the yttrium-aluminium-garnet ceramic powder chemical composition stability being prepared using this method, be single garnet structure, grain
Degree is distributed in 20-120 μm.
To achieve the above object, the present invention provides a kind of methods of low temperature synthesis yttrium-aluminium-garnet ceramic powder, including
Step: S1: rare earth oxide and aluminum contained compound are placed in agitating ball mill, with the speed ball milling 1- of 130-150r/min
2h crosses 80 meshes later, obtains powder；Wherein, rare earth oxide Y2O3Or Er2O3And Y2O3The mixture of the two；S2: by powder
Material is put into sand mill, grinds 3-4h with the revolving speed of 2200-2700r/min, filtering means dehydration and is dried later, is obtained grain diameter
For the superfine powder of 20-50nm；S3: by superfine powder 1100-1200 DEG C heat preservation 5-7 hours, obtain yttrium-aluminium-garnet ceramics
Powder.It should be noted that the Al (OH) that the present invention uses3、Al2O3、Er2O3、Y2O3Chemical purity >=99.99%.
Preferably, in S1, aluminum contained compound is Al (OH)3And/or Al2O3, preferably Al (OH)3。
Preferably, in S1, the molar ratio of rare earth oxide and aluminum contained compound is 3:10.
Preferably, in S1, in mechanical milling process: abrasive body be 8-10mm zirconia ball, decentralized medium be water preferably go from
Sub- water.
Preferably, in S1, the mass ratio of pellet is 1:(2-3), expect that the mass ratio of water is 1:(1-2).
Preferably, in S2, in process of lapping: abrasive body is the zirconium oxide bead that partial size is 0.3mm or so, and abrasive media is water
Preferably deionized water, dispersing agent are poly- methacrylate amine and/or alcohol.
Preferably, in S2, the mass ratio of pellet is 1:1.5, expects that the mass ratio of water is 1:(2-3), the dosage of dispersing agent is
The 0.7%-1.0% of powder.
Preferably, in S2, the time of drying is 18-20h.
Preferably, in S2, revolving speed is to be gradually increased to 2700r/min from 2200r/min.
The present invention also protects the yttrium-aluminium-garnet ceramic powder synthesized according to the above method.
The present invention can reduce the condition of Solid phase synthesis yttrium-aluminium-garnet, including reduce synthesis temperature, be not necessarily to vacuum gas
Atmosphere and shortening soaking time；It is garnet crystal structure and chemical composition stability using the ceramic powder that this method obtains.This
Invention uses the higher Al of reactivity (OH)3Substitute the Al in traditional preparation methods2O3.To promote solid solution reaction, material powder
Levigate to nanoscale using sand-blast, decentralized medium is deionized water, and the poly- methacrylate amine calcining of dispersing agent can remove not
It needs to wash, no waste liquid generates, and is conducive to environmental protection；Gained nanometer grade powder 1100-1200 DEG C of sintering 5-7h under normal pressure, air atmosphere
Yttrium-aluminium-garnet ceramic powder can be obtained, and without other miscellaneous phases, solid solution is good.The present invention uses general milling and high-energy ball milling
In conjunction with general milling is levigate by raw material, to reach sand mill feed size requirement, prevents coarse granule from blocking pipeline.Sand milling be by
The raw material is levigate to nano-powder, to meet solid phase reaction condition.The yttrium-aluminium-garnet ceramic powder of the method for the present invention preparation, no
It is only limitted to Er3+The Y of doping vario-property3Al5O12, further include utilizing Yb3+And Gd3+The Y of equal doping vario-properties3Al5O12, such as
(YbxY1-x)3Al5O12(GdxY1-x)3Al5O12。
Technical solution provided by the invention, with following the utility model has the advantages that (1) sand milling technology prepares superfine powder to be a kind of
Physical method, mainly broken to powder during running at high speed by ball-milling medium, the process is easy to operate, no waste liquid
It generates, meets environmental requirement；In the present invention, for material powder after being sanded, powder granularity is uniform, has high-specific surface area, high
It is easier to be sintered under temperature, energy saving, and component segregation or loss, nothing is not present during the powder handling and synthesis in solid state
Impurity introduces, and is a kind of powder processing method of environmental protection；(2)) yttrium-aluminium-garnet ceramic powder is needed using 1600 DEG C of high temperature guarantors
The special type sintering processing such as warm 20h or more, vacuum-sintering can just obtain, and vacuum-sintering equipment has at high cost, complicated for operation, energy consumption
The disadvantages of high；The powder that method provided by the invention is sanded, using normal pressure-sintered under common high temperature furnace, atmospheric environment
Obtain stablizing the ceramic powder of garnet structure, it is at low cost, it is easy to operate, it is easy to spread in industrialized production.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described.
The following examples are only intended to illustrate the technical solution of the present invention more clearly, therefore is intended only as example, and cannot be come with this
It limits the scope of the invention.
Experimental method in following embodiments is unless otherwise specified conventional method.Examination as used in the following examples
Material is tested, is to be commercially available from conventional reagent shop unless otherwise specified.Quantitative test in following embodiment, is all provided with
Three repeated experiments are set, data are the average value or mean+SD of three repeated experiments.
The present invention provides a kind of method of low temperature synthesis yttrium-aluminium-garnet ceramic powder, comprising steps of
S1: the rare earth oxide of chemical purity >=99.99% and aluminum contained compound are placed in agitating ball mill, with 130-
The speed ball milling 1-2h of 150r/min prevents coarse granule from blocking pipeline to reach sand mill feed size requirement；Agitating ball mill
Liner and stirring rod housing are all made of polyurethane material, the zirconia ball of abrasive body 8-10mm, and decentralized medium is preferably with water
Deionized water, the mass ratio of pellet are 1:(2-3), the mass ratio of water is expected for 1:(1-2), slurry crosses 80 meshes after ball milling,
Obtain powder；Wherein, rare earth oxide Y2O3Or Er2O3And Y2O3The mixture of the two；Aluminum contained compound is Al (OH)3With/
Or Al2O3, preferably Al (OH)3；The molar ratio of rare earth oxide and aluminum contained compound is 3:10；
S2: powder is put into sand mill it is further levigate to powder, ball-milling medium be water be preferably deionized water, grinding
Body is zirconium oxide bead (partial size 0.3mm or so), and material: ball: the mass ratio of water is 1:1.5:(2-3), the poly- methacrylate of dispersing agent
The dosage of amine and/or alcohol is the 0.7%-1.0% of powder；Sand mill revolving speed is gradually increased to 2700r/min by 2200r/min,
Discharge after 3-4h, to slurry filtration be dehydrated, be placed on oven drying 18-20h, obtain grain diameter be 20-50nm it is ultra-fine
Powder；
S3: by superfine powder 1100-1200 DEG C heat preservation 5-7 hours, obtaining crystal phase is single yttrium-aluminium-garnet structure
Ceramic powder.
Combined with specific embodiments below to low temperature provided by the invention synthesis yttrium-aluminium-garnet ceramic powder method make into
One step explanation.
Embodiment 1
The present embodiment provides a kind of methods of low temperature synthesis yttrium-aluminium-garnet ceramic powder, comprising steps of
S1: by the Y of chemical purity >=99.99%2O3With Al (OH)3Powder is placed in polyurethane ball milling with the molar ratio of 3:10
In tank, with the speed ball milling 1h of 130r/min, to reach sand mill feed size requirement, prevent coarse granule from blocking pipeline；Stirring
Inner liner of bowl mill and stirring rod housing are all made of polyurethane material, the zirconia ball of abrasive body 8-10mm, and decentralized medium is spent
Ionized water, the mass ratio of pellet are 1:2, expect that the mass ratio of water is 1:1, slurry crosses 80 meshes after ball milling, obtains powder；
S2: powder being put into sand mill further levigate to powder, and ball-milling medium is deionized water, and abrasive body is oxidation
Zirconium pearl (partial size 0.3mm or so), material: ball: the mass ratio of water is 1:1.5:2, and the dosage of the poly- methacrylate amine of dispersing agent is powder
The 0.7% of material；2h, 1h and 1h are ground respectively under the conditions of sand mill revolving speed is 2200r/min, 2400r/min and 2700r/min
After discharge, to slurry filtration, dehydration, be placed on oven drying 18h, obtain the superfine powder that grain diameter is 20-50nm；
S3: superfine powder is kept the temperature 7 hours at 1100 DEG C, obtains Y3Al5O12Ceramic powder.
As a result: the XRD diffraction pattern of the powder is shown as single garnet structure；The Y3Al5O12Ceramic powder chemistry at
Divide and stablize, size distribution is at 20-120 μm.
Embodiment 2
The present embodiment provides a kind of methods of low temperature synthesis yttrium-aluminium-garnet ceramic powder, comprising steps of
S1: by the Er of chemical purity >=99.99%2O3、Y2O3、Al(OH)3Powder is placed in the molar ratio of 0.9:2.1:10
In polyurethane ball-milling pot, prevent coarse granule from blocking to reach sand mill feed size requirement with the speed ball milling 2h of 150r/min
Pipeline；Agitating ball mill liner and stirring rod housing are all made of polyurethane material, the zirconia ball of abrasive body 8-10mm, dispersion
Medium deionized water, the mass ratio of pellet are 1:2.5, expect that the mass ratio of water is 1:1.5, slurry crosses 80 mesh after ball milling
Sieve, obtains powder；
S2: powder being put into sand mill further levigate to powder, and ball-milling medium is deionized water, and abrasive body is oxidation
Zirconium pearl (partial size 0.3mm or so), material: ball: the mass ratio of water is 1:1.5:2.5, and the dosage of the poly- methacrylate amine of dispersing agent is
The 0.8% of powder；Sand mill revolving speed be 2300r/min, 2500r/min and 2700r/min under the conditions of grind respectively 1h, 1h and
Discharge after 1h, to slurry filtration, dehydration, be placed on oven drying 20h, obtain grain diameter be 20-50nm superfine powder；
S3: superfine powder is kept the temperature 6 hours at 1150 DEG C, obtains (Er0.3Y0.7)3Al5O12Ceramic powder.
As a result: the XRD diffraction pattern of the powder is shown as single garnet structure；It should (Er0.3Y0.7)3Al5O12Ceramic powder
Chemical composition stability, size distribution is at 20-120 μm.
Embodiment 3
The present embodiment provides a kind of methods of low temperature synthesis yttrium-aluminium-garnet ceramic powder, comprising steps of
S1: by the Er of chemical purity >=99.99%2O3、Y2O3、Al(OH)3Powder is placed in the molar ratio of 2.1:0.9:10
In polyurethane ball-milling pot, with the speed ball milling 1.5h of 150r/min, to reach sand mill feed size requirement, prevent coarse granule stifled
Fill in pipeline；Agitating ball mill liner and stirring rod housing are all made of polyurethane material, and the zirconia ball of abrasive body 8-10mm divides
Dispersion media deionized water, the mass ratio of pellet are 1:3, expect that the mass ratio of water is 1:2, and slurry crosses 80 meshes after ball milling,
Obtain powder；
S2: powder being put into sand mill further levigate to powder, and ball-milling medium is deionized water, and abrasive body is oxidation
Zirconium pearl (partial size 0.3mm or so), material: ball: the mass ratio of water is 1:1.5:3, the poly- methacrylate amine 1.0% of dispersing agent；In sand
Mill speed be 2200r/min, 2500r/min and 2700r/min under the conditions of grind 1h, 2h and 1h respectively after discharge, to slurry
Filtering, dehydration, be placed on oven drying 18h, obtain grain diameter be 20-50nm superfine powder；
S3: superfine powder is kept the temperature 5 hours at 1200 DEG C, obtains (Er0.7Y0.3)3Al5O12Ceramic powder.
As a result: the XRD diffraction pattern of the powder is shown as single garnet structure；It should (Er0.7Y0.3)3Al5O12Ceramic powder
Chemical composition stability, size distribution is at 20-120 μm.
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.Unless specifically stated otherwise, it otherwise illustrates in these embodiments
Component and opposite step, numerical expression and the numerical value of step are not limit the scope of the invention.It is illustrated and described herein
In all examples, unless otherwise prescribed, any occurrence should be construed as merely illustratively, not as limitation, because
This, other examples of exemplary embodiment can have different values.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover in protection scope of the present invention.
Claims (10)
1. a kind of method of low temperature synthesis yttrium-aluminium-garnet ceramic powder, which is characterized in that comprising steps of
S1: rare earth oxide and aluminum contained compound are placed in agitating ball mill, with the speed ball milling 1-2h of 130-150r/min,
80 meshes are crossed later, obtain powder；Wherein, the rare earth oxide is Y2O3Or Er2O3And Y2O3The mixture of the two；
S2: the powder is put into sand mill, grinds 3-4h with the revolving speed of 2200-2700r/min, filtering means dehydration and is dried later
It is dry, obtain the superfine powder that grain diameter is 20-50nm；
S3: by the superfine powder 1100-1200 DEG C heat preservation 5-7 hours, obtain yttrium-aluminium-garnet ceramic powder.
2. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S1, the aluminum contained compound is Al (OH)3And/or Al2O3, preferably Al (OH)3。
3. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S1, the molar ratio of the rare earth oxide and the aluminum contained compound is 3:10.
4. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S1, in the mechanical milling process: abrasive body is 8-10mm zirconia ball, and decentralized medium is that water is preferably deionization
Water.
5. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S1, the mass ratio of pellet is 1:(2-3), expect that the mass ratio of water is 1:(1-2).
6. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S2, in the process of lapping: abrasive body is zirconium oxide bead, and abrasive media is that water is preferably deionized water, dispersion
Agent is poly- methacrylate amine and/or alcohol.
7. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 6, it is characterised in that:
In the S2, the mass ratio of pellet is 1:1.5, expects that the mass ratio of water is 1:(2-3), the dosage of the dispersing agent is described
The 0.7%-1.0% of powder.
8. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S2, the time of the drying is 18-20h.
9. the method for low temperature synthesis yttrium-aluminium-garnet ceramic powder according to claim 1, it is characterised in that:
In the S2, the revolving speed is to be gradually increased to 2700r/min from 2200r/min.
10. the yttrium-aluminium-garnet ceramic powder that any method of claim 1-9 synthesizes.
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| CN116655366A (en) * | 2023-04-17 | 2023-08-29 | 内蒙古科技大学 | Low-temperature solid-phase synthesis method of L/B-site co-doped yttrium aluminum garnet powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111266162A (en) * | 2020-03-25 | 2020-06-12 | 长沙矿冶研究院有限责任公司 | Preparation method of nano silicon powder |
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| CN116655366A (en) * | 2023-04-17 | 2023-08-29 | 内蒙古科技大学 | Low-temperature solid-phase synthesis method of L/B-site co-doped yttrium aluminum garnet powder |
| CN116655366B (en) * | 2023-04-17 | 2024-10-01 | 内蒙古科技大学 | Low-temperature solid-phase synthesis of L/B-site co-doped yttrium aluminum garnet powder |
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